Preparation and separation process of a glue peptide for tonifying qi and blood

Abstract

The application discloses a preparation and separation process of agelapeptide for tonifying qi and blood, which comprises a shell, a plurality of filter cartridges arranged uniformly in the circumferential direction are arranged in the shell, a horizontal partition plate is fixed to the middle part of the inside of each filter cartridge, a filter membrane roll is vertically arranged at the center position of the partition plate, a discharge cylinder penetrating to the outside of the bottom of the filter cartridge is fixedly connected below the filter membrane roll, a liquid inlet is formed in the sidewall of the filter cartridge above the partition plate, a liquid outlet is formed in the bottom of the filter cartridge, and a collecting cylinder is arranged below each discharge cylinder. Compared with the prior art, the agelapeptide for tonifying qi and blood has the characteristics of multistage continuous screening, automatic scraping membrane discharging and anti-deformation structure, and has significant advantages in separation efficiency, product purity and production cost control.

Description

Technical Field

[0001] This invention relates to the field of membrane separation technology, specifically a separation process for preparing donkey-hide gelatin peptides that replenish qi and blood. Background Technology

[0002] Donkey-hide gelatin, a key ingredient in traditional Chinese medicine, is made primarily from donkey skin and is known for its effects of replenishing qi and blood, nourishing yin, and moisturizing dryness. However, the large-molecule collagen in traditional donkey-hide gelatin is difficult for the human body to absorb directly, resulting in low bioavailability. By using enzymatic or chemical hydrolysis processes to break down large-molecule collagen into small-molecule active peptides (i.e., donkey-hide gelatin peptides), its absorption rate and bioactivity can be significantly improved. Studies have shown that donkey-hide gelatin peptides not only retain the blood-replenishing effects of traditional donkey-hide gelatin but also possess new functions such as anti-oxidation and immune regulation, making them widely applicable in the development of health products, functional foods, and pharmaceuticals.

[0003] Currently, the separation and purification of donkey-hide gelatin peptides mainly rely on the following methods: centrifugation, which separates components of different molecular weights through centrifugal force, but can only roughly separate large particle impurities and cannot achieve precise molecular weight fractionation; multiple centrifugation operations are time-consuming and energy-intensive, and active peptides are easily denatured and inactivated by mechanical shear force. Single-stage membrane filtration technology uses a single-pore size filter membrane to retain specific molecular weight peptides, but can only separate 1-2 target components; multi-stage sieving requires multiple devices in series, making the system complex; the filter membrane is prone to clogging, requiring frequent shutdowns for cleaning or replacement, resulting in low production efficiency; residual peptides on the membrane surface are difficult to recover completely, causing resource waste. Mechanical scraping can remove residues on the filter membrane surface, but because the filter membrane is elastic, the scraper does not adhere tightly to the filter membrane, resulting in incomplete scraping; the filter membrane support structure is weak and prone to deformation after long-term use, affecting separation accuracy.

[0004] Therefore, it is necessary to provide a preparation and separation process for donkey-hide gelatin peptides that replenish qi and blood, in order to solve the problems mentioned in the background art. Summary of the Invention

[0005] To achieve the above objectives, the present invention provides the following technical solution:

[0006] A preparation and separation process for a blood-tonifying donkey-hide gelatin peptide includes the following steps:

[0007] S1. Raw material pretreatment: Crush the donkey-hide gelatin raw material to a particle size ≤1mm, add deionized water at a material-to-liquid ratio of 1:10-1:15, stir to dissolve, adjust the pH to 6.5-7.5, heat to 50-60℃ and keep warm for 30-40 minutes, centrifuge to remove insoluble matter, and obtain crude extract of donkey-hide gelatin.

[0008] S2. Enzymatic hydrolysis: Add a complex protease to the crude extract of donkey-hide gelatin. The complex protease is a mixture of trypsin and neutral protease in a mass ratio of 1:2 to 1:3. The enzymatic hydrolysis temperature is 45-55℃ and the enzymatic hydrolysis time is 4-6 hours. After enzymatic hydrolysis, the enzyme is inactivated to obtain the enzymatic hydrolysate.

[0009] S3. Multistage membrane separation: The enzymatic hydrolysate is pumped into a multistage membrane separation device and sequentially passed through 10kDa, 7kDa, 4kDa, and 1kDa filter membranes for fractional retention. The operating pressure is controlled at 0.2-0.5MPa and the flow rate at 3-5L / min. The active peptide components at each stage are collected separately.

[0010] S4. Drying and purification: The active peptide components at all levels are concentrated under vacuum to a solid content of ≥30%, and spray-dried at an inlet air temperature of 160-180℃ and an outlet air temperature of 70-90℃ to obtain donkey-hide gelatin peptide powder with a purity of ≥90%.

[0011] The multi-stage membrane separation unit in S3 includes:

[0012] The outer shell contains multiple filter cartridges arranged evenly along the circumference inside.

[0013] A horizontal partition is fixed in the middle of the interior of each filter cylinder, and a filter membrane roll is vertically arranged at the center of the partition. A discharge cylinder that extends to the bottom outside of the filter cylinder is fixedly connected below the filter membrane roll.

[0014] The filter cylinder above the partition has an inlet on its side wall and an outlet at its bottom.

[0015] A collection cylinder is placed below each of the discharge cylinders.

[0016] Furthermore, as a preferred embodiment, each of the discharge cylinders is provided with a baffle at its upper end, and a rotating shaft is fixed at the center of the baffle, the rotating shaft being rotatably connected to the side wall of the discharge cylinder.

[0017] Furthermore, preferably, one end of the rotating shaft rotatably passes through the side wall of the discharge cylinder and the filter cylinder, and is fixed with a driven bevel gear. A driving bevel gear is provided inside the housing, and the driving bevel gear meshes with each driven bevel gear.

[0018] Furthermore, as a preferred embodiment, each of the filter cartridges is slidably provided with a piston, and the liquid inlet is provided with a one-way valve that allows liquid to flow in but not out.

[0019] Furthermore, as a preferred embodiment, each piston is rotatably provided with a rotating block at its center, and a plurality of vertically arranged scrapers are fixed below the rotating block.

[0020] Furthermore, preferably, a connecting shaft is fixed above each of the rotating blocks, the connecting shaft extends through to the top of the filter cylinder, a connecting plate is provided above the filter cylinder, and each connecting shaft is rotatably connected to the connecting plate;

[0021] Each of the connecting shafts has a driven gear fixed at its upper end, and a driving gear is provided at the center of the connecting disc. The driving gear meshes with each of the driven gears.

[0022] Furthermore, as a preferred embodiment, a top lifting cylinder is provided on the top of the housing, and the piston rod of the top lifting cylinder is fixed to the connecting plate.

[0023] Furthermore, preferably, multiple reinforcing ribs are attached and fixed to the outer wall of the filter membrane roll, and the upper ends of the reinforcing ribs are fixed to the partition.

[0024] Furthermore, as a preferred embodiment, the outer wall of the discharge cylinder has multiple bonding plates distributed along the gaps of the reinforcing ribs, and the outer wall of the discharge cylinder is also slidably provided with a slip ring, with the bottom of the bonding plate fixed to the slip ring.

[0025] Furthermore, as a preferred embodiment, a lifting plate is provided at the lower part of the outer casing, and a bottom lifting cylinder is provided between the lifting plate and the bottom of the outer casing;

[0026] Each slip ring is fixed with a guide shaft below it, and each guide shaft passes through the lower end of the filter cylinder and is fixed to the lifting plate.

[0027] Compared with the prior art, the beneficial effects of the present invention are:

[0028] In this invention, by using multiple filter cylinders connected in series and filter membrane pore sizes that decrease progressively, continuous multi-stage sieving of the molecular weight of the donkey-hide gelatin peptide solution can be achieved, and various active peptides with different molecular weights can be separated.

[0029] In this invention, the meshing of a drive gear and a driven gear enables all scrapers to rotate synchronously, rapidly stripping away peptides trapped on the filter membrane surface. The filter membrane roll, aided by a bonding plate, ensures it remains taut during scraper operation, allowing for proper contact between the scraper and the membrane roll and preventing pore size deviations caused by deformation. A bevel gear-driven control system opens and closes the baffle, eliminating the need for manual intervention during the discharge process and avoiding the time-consuming nature of traditional filter membrane cleaning.

[0030] In this invention, a piston allows the hydrolyzed donkey-hide gelatin peptide solution to pass through a filter membrane roll under pressure, improving filtration efficiency. The rising piston, combined with the sealing effect of the bonding plate, creates a stable negative pressure, ensuring efficient solution intake and uniform distribution. Attached Figure Description

[0031] Figure 1 A flowchart illustrating the preparation and separation process of a blood-tonifying donkey-hide gelatin peptide;

[0032] Figure 2 This is a schematic diagram of the internal structure of a multi-stage membrane separation device;

[0033] Figure 3 This is a schematic cross-sectional view of a multi-stage membrane separation device.

[0034] Figure 4 This is a top view schematic diagram of a multi-stage membrane separation device;

[0035] Figure 5 This is a schematic diagram of the internal structure of the filter cartridge;

[0036] Figure 6 This is a schematic diagram of the cross-sectional structure of the filter cartridge;

[0037] In the diagram: 1. Outer shell; 2. Filter cylinder; 201. Partition plate; 202. Filter membrane roll; 203. Discharge cylinder; 204. Baffle plate; 205. Piston; 206. Rotating block; 207. Scraper; 208. Liquid inlet; 209. Liquid outlet; 210. Rotating shaft; 211. Reinforcing rib; 212. Adhesive plate; 213. Slip ring; 214. Guide shaft; 215. Driven bevel gear; 216. Driven bevel gear; 3. Collection cylinder; 4. Connecting pipe; 5. Connecting shaft; 6. Connecting disc; 7. Driven gear; 8. Driven gear; 9. Top lifting cylinder; 10. Lifting disc; 11. Bottom lifting cylinder. Detailed Implementation

[0038] Please see Figures 1-6 In this embodiment of the invention, a preparation and separation process for a blood-tonifying donkey-hide gelatin peptide is characterized by comprising the following steps:

[0039] S1. Raw material pretreatment: Crush the donkey-hide gelatin raw material to a particle size ≤1mm, add deionized water at a material-to-liquid ratio of 1:10-1:15, stir to dissolve, adjust the pH to 6.5-7.5, heat to 50-60℃ and keep warm for 30-40 minutes, centrifuge to remove insoluble matter, and obtain crude extract of donkey-hide gelatin.

[0040] S2. Enzymatic hydrolysis: Add a complex protease to the crude extract of donkey-hide gelatin. The complex protease is a mixture of trypsin and neutral protease in a mass ratio of 1:2 to 1:3. The enzymatic hydrolysis temperature is 45-55℃ and the enzymatic hydrolysis time is 4-6 hours. After enzymatic hydrolysis, the enzyme is inactivated to obtain the enzymatic hydrolysate.

[0041] S3. Multistage membrane separation: The enzymatic hydrolysate is pumped into a multistage membrane separation device and sequentially passed through 10kDa, 7kDa, 4kDa, and 1kDa filter membranes for fractional retention. The operating pressure is controlled at 0.2-0.5MPa and the flow rate at 3-5L / min. The active peptide components at each stage are collected separately.

[0042] S4. Drying and purification: The active peptide components at all levels are concentrated under vacuum to a solid content of ≥30%, and spray-dried at an inlet air temperature of 160-180℃ and an outlet air temperature of 70-90℃ to obtain donkey-hide gelatin peptide powder with a purity of ≥90%.

[0043] The multi-stage membrane separation unit in S3 includes:

[0044] The outer shell 1 has multiple filter cylinders 2 arranged evenly along the circumference inside it;

[0045] A horizontal partition 201 is fixed in the middle of the interior of each filter cylinder 2. A filter membrane roll 202 is vertically arranged at the center of the partition 201. A discharge cylinder 203 that extends to the bottom outside of the filter cylinder 2 is fixedly connected below the filter membrane roll 202.

[0046] The filter cylinder 2 above the partition 201 has an inlet 208 on its side wall and an outlet 209 at its bottom.

[0047] A collection cylinder 3 is placed below each of the discharge cylinders 203.

[0048] The multiple filter cylinders 2 are connected in series: the inlet 208 of the first filter cylinder 2 is connected to the supply pipeline of the hydrolyzed donkey-hide gelatin peptide solution, the inlet 208 of the remaining filter cylinders 2 are respectively connected to the outlet 209 of the previous filter cylinder 2, and the outlet 209 of the last filter cylinder 2 is connected to the waste liquid collection device.

[0049] The pore size of each filter membrane roll 202 decreases progressively along the liquid flow direction, which is used to perform multi-stage sieving of peptides in the donkey-hide gelatin peptide solution according to molecular weight.

[0050] In this embodiment, each discharge cylinder 203 is provided with a baffle 204 at its upper end, and a rotating shaft 210 is fixed at the center of the baffle 204. The rotating shaft 210 is rotatably connected to the side wall of the discharge cylinder 203.

[0051] In this embodiment, one end of the rotating shaft 210 rotatably passes through the side wall of the discharge cylinder 203 and the filter cylinder 2, and is fixed with a driven bevel gear 215. A drive bevel gear 216 is provided inside the outer casing 1, and the drive bevel gear 216 meshes with each driven bevel gear 215.

[0052] By driving the bevel gear 216, each driven bevel gear 215 can be rotated, thereby controlling the opening and closing of each baffle 204. When the filter membrane roll 202 has completed filtration, the peptide segments left in the filter membrane roll 202 can be discharged from the discharge cylinder 203 to the collection cylinder 3 by opening the baffle 204.

[0053] In this embodiment, a piston 205 is slidably disposed inside each of the filter cartridges 2, and a one-way valve that allows only liquid to enter and not exit is disposed in the liquid inlet 208.

[0054] When piston 205 slides upward, the donkey-hide gelatin peptide solution can be drawn from the supply pipe or connecting pipe 4 into the upper part of the inner partition 201 of the filter cartridge 2.

[0055] In this embodiment, each piston 205 is rotatably provided with a rotating block 206 at its center, and a plurality of vertically arranged scrapers 207 are fixed below the rotating block 206.

[0056] When the piston 205 descends to be in contact with the partition 201, the rotating block 206 can be rotated to make the scraper 207 move in a circular motion on the inner wall of the filter membrane roll 202, thereby detaching the peptide segments from the inner wall of the filter membrane roll 202 and discharging them from the discharge cylinder 203.

[0057] In this embodiment, a connecting shaft 5 is fixed above each of the rotating blocks 206, the connecting shaft 5 extends through the top of the filter cylinder 2, a connecting plate 6 is provided above the filter cylinder 2, and each connecting shaft 5 is rotatably connected to the connecting plate 6;

[0058] Each of the connecting shafts 5 has a driven gear 7 fixed at its upper end, and a drive gear 8 is provided at the center of the connecting disc 6. The drive gear 8 meshes with each of the driven gears 7.

[0059] In other words, the drive gear 8 can drive each driven gear 7 to rotate, thereby controlling the rotation of each rotating block 206.

[0060] In this embodiment, a top lifting cylinder 9 is provided on the top of the outer casing 1, and the piston rod of the top lifting cylinder 9 is fixed to the connecting plate 6.

[0061] The lifting cylinder 9 at the top can drive the connecting plate 6 to rise and fall, thereby controlling the rise and fall of each piston 205.

[0062] In this embodiment, multiple reinforcing ribs 211 are attached and fixed to the outer wall of the filter membrane roll 202, and the upper end of the reinforcing ribs 211 is fixed to the partition plate 201.

[0063] The reinforcing ribs 211 can maintain the tension of the filter membrane roll 202, ensuring that it remains taut.

[0064] In this embodiment, multiple bonding plates 212 are distributed along the gaps of the reinforcing ribs 211 on the outer wall of the discharge cylinder 203, and a slip ring 213 is slidably provided on the outer wall of the discharge cylinder 203, with the bottom of the bonding plate 212 fixed in the slip ring 213.

[0065] In this embodiment, a lifting plate 10 is provided at the lower part of the outer shell 1, and a bottom lifting cylinder 11 is provided between the lifting plate 10 and the bottom of the outer shell 1;

[0066] Each slip ring 213 is fixed with a guide shaft 214 below it, and each guide shaft 214 passes through the lower end of the filter cylinder 2 and is fixed to the lifting plate 10.

[0067] The bottom lifting cylinder 11 can drive the lifting plate 10 to move up and down, thereby controlling the sliding of each slip ring 213, so that the bonding plate 212 can be bonded to the outer wall of the filter membrane roll 202 along the gap of the reinforcing rib 211. When the scraper 207 moves in a circular motion on the inner wall of the filter membrane roll 202 to scrape off the peptide segments, the filter membrane roll 202 is fixed in position under the action of the bonding plate 212, so that it can be tightly bonded to the scraper 207. In addition, when the piston 205 moves up, the bonding plate 212 can seal the filter membrane roll 202 to ensure that negative pressure is generated at the liquid inlet 208.

[0068] In practice, the multi-stage membrane separation process includes:

[0069] The top lifting cylinder 9 drives the connecting plate 6 to drive all pistons 205 to rise synchronously. When the pistons rise, the one-way valve opens, and the solution is sequentially drawn into the upper chamber of each filter cartridge partition 201 through the liquid inlet 208.

[0070] The top lifting cylinder 9 drives the connecting plate 6 to drive all pistons 205 to descend synchronously to fit with the partition 201. During the process, the solution passes through the filter membrane roll 202 under the action of gravity and pressure. Large molecular peptides are trapped on the inner wall of the first-stage filter membrane, and small molecules enter the next stage. Each stage of filter membrane traps peptides of the corresponding molecular weight range, and the final filtrate is discharged as waste liquid.

[0071] The lifting plate 10 is driven to rise by the bottom lifting cylinder 11, so that the bonding plate 212 rises along the gap of the reinforcing rib 211 to ensure close contact with the outer wall of the filter membrane roll.

[0072] The drive bevel gear 216 rotates, which in turn drives the driven bevel gear 215 to open the baffle 204, starts the drive gear 8, and drives all rotating blocks 206 and scraper 207 to rotate, scraping the peptide segments on the inner wall of the filter membrane into the discharge cylinder 203.

[0073] The above description is merely a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.

Claims

1. A preparation and separation process for a blood-tonifying donkey-hide gelatin peptide, characterized in that, Includes the following steps: S1. Raw material pretreatment: Crush the donkey-hide gelatin raw material to a particle size ≤1mm, add deionized water at a material-to-liquid ratio of 1:10-1:15, stir to dissolve, adjust the pH to 6.5-7.5, heat to 50-60℃ and keep warm for 30-40 minutes, centrifuge to remove insoluble matter, and obtain crude extract of donkey-hide gelatin. S2. Enzymatic hydrolysis: Add a complex protease to the crude extract of donkey-hide gelatin. The complex protease is a mixture of trypsin and neutral protease in a mass ratio of 1:2 to 1:

3. The enzymatic hydrolysis temperature is 45-55℃ and the enzymatic hydrolysis time is 4-6 hours. After enzymatic hydrolysis, the enzyme is inactivated to obtain the enzymatic hydrolysate. S3. Multistage membrane separation: The enzymatic hydrolysate is pumped into a multistage membrane separation device and sequentially passed through 10kDa, 7kDa, 4kDa, and 1kDa filter membranes for fractional retention. The operating pressure is controlled at 0.2-0.5MPa and the flow rate at 3-5L / min. The active peptide components at each stage are collected separately. S4. Drying and purification: The active peptide components at all levels are concentrated under vacuum to a solid content of ≥30%, and spray-dried at an inlet air temperature of 160-180℃ and an outlet air temperature of 70-90℃ to obtain donkey-hide gelatin peptide powder with a purity of ≥90%. The multi-stage membrane separation unit in S3 includes: The outer shell (1) has multiple filter cylinders (2) arranged evenly in a circumferential direction inside it; A horizontal partition (201) is fixed in the middle of the interior of each filter cylinder (2). A filter membrane roll (202) is vertically arranged at the center of the partition (201). A discharge cylinder (203) that extends through to the outside of the bottom of the filter cylinder (2) is fixedly connected below the filter membrane roll (202). The filter cylinder (2) above the partition (201) has an inlet (208) on its side wall and an outlet (209) at its bottom. A collection cylinder (3) is placed below each of the discharge cylinders (203); Each of the discharge cylinders (203) is provided with a baffle (204) at its upper end, and a rotating shaft (210) is fixed at the center of the baffle (204); A piston (205) is slidably disposed inside each of the filter cylinders (2), and a rotating block (206) is rotatably disposed at the center of each piston (205). A plurality of vertically disposed scrapers (207) are fixed below the rotating block (206). The outer wall of the filter membrane roll (202) is fixed with multiple reinforcing ribs (211), and the outer wall of the discharge cylinder (203) is distributed with multiple bonding plates (212) along the gaps of the reinforcing ribs (211). The outer wall of the discharge cylinder (203) is also slidably provided with a slip ring (213), and the bottom of the bonding plate (212) is fixed in the slip ring (213).

2. The preparation and separation process of a qi- and blood-tonifying donkey-hide gelatin peptide according to claim 1, characterized in that, The rotating shaft (210) is rotatably connected to the side wall of the discharge cylinder (203).

3. The preparation and separation process of a qi- and blood-tonifying donkey-hide gelatin peptide according to claim 2, characterized in that, One end of the rotating shaft (210) rotatably passes through the side wall of the discharge cylinder (203) and the filter cylinder (2), and is fixed with a driven bevel gear (215). A drive bevel gear (216) is provided inside the outer shell (1), and the drive bevel gear (216) meshes with each driven bevel gear (215).

4. The preparation and separation process of a qi- and blood-tonifying donkey-hide gelatin peptide according to claim 1, characterized in that, The inlet (208) is equipped with a one-way valve that allows only liquid to enter and not exit.

5. The preparation and separation process of a qi- and blood-tonifying donkey-hide gelatin peptide according to claim 1, characterized in that, Each of the rotating blocks (206) is fixed with a connecting shaft (5) above it. The connecting shaft (5) extends through the filter cylinder (2) above it. A connecting plate (6) is provided above the filter cylinder (2). Each of the connecting shafts (5) is rotatably connected to the connecting plate (6). Each of the connecting shafts (5) has a driven gear (7) fixed at its upper end, and a drive gear (8) is provided at the center of the connecting disc (6), and the drive gear (8) meshes with each of the driven gears (7).

6. The preparation and separation process of a qi- and blood-tonifying donkey-hide gelatin peptide according to claim 5, characterized in that, The top of the outer casing (1) is provided with a top lifting cylinder (9), and the piston rod of the top lifting cylinder (9) is fixed to the connecting plate (6).

7. The preparation and separation process of a qi- and blood-tonifying donkey-hide gelatin peptide according to claim 1, characterized in that, The upper end of the reinforcing rib (211) is fixed to the partition plate (201).

8. The preparation and separation process of a qi- and blood-tonifying donkey-hide gelatin peptide according to claim 7, characterized in that, A lifting plate (10) is provided at the bottom inside the outer shell (1), and a bottom lifting cylinder (11) is provided between the lifting plate (10) and the bottom of the outer shell (1); Each slip ring (213) is fixed with a guide shaft (214) below it, and each guide shaft (214) passes through the lower end of the filter cylinder (2) and is fixed to the lifting plate (10).

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